WO2023090111A1 - 成分濃度測定装置、成分濃度測定プログラム、及び、成分濃度測定方法 - Google Patents

成分濃度測定装置、成分濃度測定プログラム、及び、成分濃度測定方法 Download PDF

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WO2023090111A1
WO2023090111A1 PCT/JP2022/040152 JP2022040152W WO2023090111A1 WO 2023090111 A1 WO2023090111 A1 WO 2023090111A1 JP 2022040152 W JP2022040152 W JP 2022040152W WO 2023090111 A1 WO2023090111 A1 WO 2023090111A1
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concentration
component
liquid sample
measured
conductivity
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English (en)
French (fr)
Japanese (ja)
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達也 中原
拓也 斧田
一徳 土生
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Horiba Advanced Techno Co Ltd
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Horiba Advanced Techno Co Ltd
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Priority to CN202280073109.0A priority Critical patent/CN118215836A/zh
Priority to US18/702,053 priority patent/US20250044209A1/en
Priority to JP2023561498A priority patent/JPWO2023090111A1/ja
Priority to KR1020247012905A priority patent/KR20240112258A/ko
Publication of WO2023090111A1 publication Critical patent/WO2023090111A1/ja
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • G01N15/075—Investigating concentration of particle suspensions by optical means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • G01N15/0656—Investigating concentration of particle suspensions using electric, e.g. electrostatic methods or magnetic methods
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/59—Transmissivity
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/27—Association of two or more measuring systems or cells, each measuring a different parameter, where the measurement results may be either used independently, the systems or cells being physically associated, or combined to produce a value for a further parameter
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/302—Electrodes, e.g. test electrodes; Half-cells pH sensitive, e.g. quinhydron, antimony or hydrogen electrodes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • G01N2015/0687—Investigating concentration of particle suspensions in solutions, e.g. non volatile residue

Definitions

  • the present invention relates to a component concentration measuring device for measuring the concentration of a component to be measured in a liquid sample, a component concentration measuring program, and a component concentration measuring method.
  • absorption spectroscopy is used as shown in Patent Document 1 as a method for measuring the concentration of a measurement target component contained in a liquid sample such as a chemical solution.
  • a liquid sample is irradiated with light to measure a light absorption spectrum (spectral spectrum), and the absorbance obtained from the light absorption spectrum is converted into a concentration using a previously obtained calibration curve. .
  • the above absorption spectroscopy has the problem of large instrumental differences in principle.
  • the instrumental difference is a difference in measured values that occurs between apparatuses of the same model.
  • causes of instrumental differences include variation in light source intensity, variation in detector sensitivity, and variation in mechanical accuracy of optical systems among devices.
  • a liquid sample contains a plurality of components and the absorption spectra of these components overlap each other, it is difficult to accurately measure the concentration of the component to be measured.
  • concentration measurement of trace components at the ppm level is required, and importance is attached to improving the accuracy of concentration measurement of components to be measured.
  • the present invention has been made to solve the above-mentioned problems, and the main object thereof is to accurately determine the concentration of the component to be measured contained in the liquid sample.
  • a component concentration measuring device measures the concentration of a component to be measured contained in a liquid sample, and includes an optical measurement unit for measuring the spectrum of the liquid sample, and a characteristic value of the liquid sample. It is characterized by comprising an electrochemical measurement unit that performs electrochemical measurement, and a concentration calculation unit that calculates the concentration of the component to be measured by multivariate analysis using the spectroscopic spectrum and the characteristic value as explanatory variables.
  • the concentration of the component to be measured is calculated by multivariate analysis using the spectroscopic spectrum of the liquid sample and the characteristic value of the liquid sample as explanatory variables. can be obtained with high accuracy.
  • characteristic values obtained by electrochemical measurement which is a measurement method with little instrumental difference in principle, are used as explanatory variables for multivariate analysis, so only absorption spectroscopy is used.
  • the concentration calculation unit performs primary differentiation or secondary differentiation of the spectral spectrum with respect to wavelength, and performs multivariate analysis using the differential value as an explanatory variable. It is desirable to be With this configuration, the measurement accuracy of the measurement target component can be improved compared to the case of using the absorbance at one wavelength. Note that when using the absorbance at one wavelength, the data is only for one point and is not a continuous function, so differentiation processing cannot be performed, and the influence of drift due to light source fluctuations and stray light must be reduced. is difficult.
  • the SN ratio is better than when second-order differentiation is performed.
  • the concentration calculation unit performs multivariate analysis using values at at least one or more wavelengths in the spectral spectrum as explanatory variables.
  • the electrochemical measurement unit may have a conductivity meter that measures the conductivity of the liquid sample or a pH meter that measures the pH of the liquid sample. desirable.
  • This conductivity meter and pH meter have small instrumental differences due to the measurement principle, and by adding these to the explanatory variables of multivariate analysis, compared to the case of calculating the concentration of the measurement target component using only absorption spectroscopy Machine difference can be reduced.
  • a conductivity meter is desirable, and if the liquid sample contains a trace component correlated with hydrogen ions (H + ), a pH meter is recommended. It is desirable to have
  • the electrochemical measurement unit is configured to measure the conductivity of the liquid sample. It is desirable to have a rate meter and a pH meter for measuring the pH of the liquid sample, and the concentration calculator to calculate the concentration of the component to be measured by multivariate analysis using the following formula.
  • the electrochemical measurement unit has a conductivity meter, the component that produces conductivity in the spectroscopic spectrum and components that do not produce conductivity are superimposed, they can be measured separately.
  • the explanatory variable of conductivity even for components that are indistinguishable only by spectroscopic spectra (even for samples whose concentration cannot be measured for each component by spectroscopic spectra alone)
  • the weighting of each explanatory variable that describes the component concentration is changed. This makes it possible to measure the concentration of each of the components whose absorption spectra overlap and cannot be separated.
  • the curve represents the absorbance of the sample
  • the round points of conductivity and pH represent the respective measured values
  • the bar graph quantifies the magnitude of the effect of each explanatory variable on the concentration. (displayed as "concentration contribution rate” in the figure).
  • the electrochemical measurement unit has a pH meter
  • hydrogen Even if a component correlated with ions and a component uncorrelated with hydrogen ions are superimposed, they can be separated and measured. Specifically, as shown in Fig. 3, by increasing the pH explanatory variable, even for components that cannot be distinguished by spectroscopic spectra alone (even in samples whose concentrations cannot be measured for each component by spectroscopic spectra alone), the component The weighting of each explanatory variable that explains the concentration (the equivalent of the concentration regression coefficient for each explanatory variable) is changed. This makes it possible to measure the concentration of each of the components whose absorption spectra overlap and cannot be separated.
  • a component concentration measurement program measures the concentration of a component to be measured contained in a liquid sample, and includes an optical measurement unit for measuring the spectrum of the liquid sample, and a characteristic of the liquid sample.
  • An electrochemical measuring unit that electrochemically measures a value
  • a concentration calculating unit that calculates the concentration of the measurement target component by multivariate analysis using the spectroscopic spectrum and the characteristic value as explanatory variables. do.
  • a component concentration measuring method is a method for measuring the concentration of a component to be measured contained in a liquid sample, wherein the spectroscopic spectrum of the liquid sample is measured, and the characteristic value of the liquid sample is electrochemically measured. and calculating the concentration of the component to be measured by multivariate analysis using the spectroscopic spectrum and the characteristic value as explanatory variables.
  • the concentration of the measurement target component of the liquid sample can be determined with high accuracy by multivariate analysis using the spectroscopic spectrum of the liquid sample and the characteristic values of the liquid sample as explanatory variables.
  • FIG. 1 is a schematic diagram showing the configuration of a component concentration measuring device according to an embodiment of the present invention
  • FIG. It is experimental data showing the effect of instrumental error between (a) the case of using the calibration curve of the conventional example and (b) the case of using the calibration curve of the present embodiment.
  • a component concentration measuring device 100 measures the concentration of a component to be measured contained in a liquid sample such as a chemical solution used in semiconductor manufacturing equipment.
  • This component concentration measuring device 100 is interposed, for example, in a chemical pipe that supplies the chemical, and measures the concentration of the component to be measured in the chemical. By using the concentration thus obtained, the concentration and the like of the chemical solution are controlled.
  • the chemical solution is a mixed chemical solution (mixed liquid sample) of two or more components, for example, a component that produces conductivity when dissolved, a component that does not produce conductivity, or a component that correlates with hydrogen ions (H + ). contains.
  • the component concentration measuring device 100 includes an optical measuring unit 2 for measuring the spectroscopic spectrum of a liquid sample, an electrochemical measuring unit 3 for electrochemically measuring characteristic values of the liquid sample, An information processing device 4 for processing measurement information obtained from the optical measurement unit 2 and the electrochemical measurement unit 3 is provided.
  • the characteristic value is a physical property value that correlates with the concentration of the component to be measured contained in the liquid sample.
  • the optical measurement unit 2 is an absorbance meter that irradiates a liquid sample with light and measures the absorbance of the liquid sample.
  • the optical measurement unit 2 includes a flow cell 21 through which a liquid sample flows, a light irradiation unit 22 having a light source 22a for irradiating the liquid sample in the flow cell 21 with light, a condenser lens 22b, and the like, It has a photodetector 23 having a spectrometer 23a that disperses and detects light, a photodetector 23b, and the like.
  • a light absorption spectrum (spectral spectrum) of the transmitted light is obtained by the light detection unit 23 .
  • the light absorption spectrum of the present embodiment is a concept including an absorbance spectrum obtained from the light absorption spectrum of transmitted light and the light absorption spectrum of incident light.
  • the flow cell 21 is provided in a first sample channel L1 formed by a chemical pipe (not shown) connected to the chemical tank 5 of the semiconductor manufacturing apparatus, for example.
  • the electrochemical measurement unit 3 of this embodiment includes a conductivity meter 31 that measures the conductivity (electrical conductivity) of the liquid sample and a pH meter 32 that measures the pH of the liquid sample.
  • the conductivity meter 31 applies an alternating voltage between two electrodes 31a and 31b and measures the conductivity (electrical conductivity) of the liquid sample based on the flowing current.
  • the conductivity meter 31 of this embodiment is provided upstream or downstream of the optical measurement section 2 in the first sample flow path L1 in which the optical measurement section 2 is provided.
  • the conductivity meter 31 may be of an AC 4-pole type, or of an electromagnetic induction type, instead of an AC 2-pole type.
  • the conductivity meter 31 may be provided in a sample channel different from the first sample channel L1.
  • the pH meter 32 measures the pH of the liquid sample based on the potential difference generated between the pH glass electrode (working electrode) 32a and the reference electrode 32b.
  • the pH meter 32 of this embodiment is provided in a second sample channel L2 formed by a chemical pipe (not shown) connected to the chemical tank 5, separately from the first sample channel L1.
  • the pH meter 32 may be provided, for example, upstream or downstream of the optical measurement section 2 in the first sample flow path L1.
  • the information processing device 4 uses the light absorption spectrum (or absorbance spectrum) obtained by the optical measurement unit 2, the conductivity obtained by the conductivity meter 31, and the pH obtained by the pH meter to measure the liquid sample is used to calculate the concentration of the component to be measured.
  • the information processing device 4 is a computer having a CPU, a memory, an input/output interface, an AD converter, output means such as a display, and input means such as a keyboard. Then, based on the component concentration calculation program stored in the memory, the CPU and the peripheral device work together to function as the concentration calculator 41 .
  • the concentration calculator 41 calculates the concentration of the component to be measured by multivariate analysis using the light absorption spectrum and characteristic values (conductivity and pH) as explanatory variables.
  • Multivariate analysis may include multiple regression analysis (MLR or ILS), principal component regression analysis (PCR), least squares method (CLS), partial least squares method (PLS (PLS1 or PLS2)), and the like.
  • the concentration calculation unit 41 differentiates the light absorption spectrum by first-order differentiation or second-order differentiation, and performs multivariate analysis using the differential value as an explanatory variable. Further, the concentration calculator 41 performs multivariate analysis using the respective values of a plurality of wavelengths in the light absorption spectrum as explanatory variables.
  • the concentration calculation unit 41 calculates the concentration of the component to be measured by multivariate analysis using the following formula.
  • Abs i is obtained by differentiating the light absorption spectrum, and is a value for each of a plurality of wavelengths ( ⁇ 1, ⁇ 2, . . . ⁇ n).
  • Coefficients a i , b, and c are respectively a concentration regression coefficient for wavelength ⁇ i, a concentration regression coefficient for conductivity, and a concentration regression coefficient for pH. Note that the concentration regression coefficient corresponds to the weight of each explanatory variable.
  • k is a calibration curve obtained in advance
  • S is measurement data (actual measurement data) of the liquid sample of the optical measurement unit 2 and the electrochemical measurement unit 3 .
  • the calibration curve is obtained by performing multivariate analysis using the above equation on the measurement data of the optical measurement unit 2 and the electrochemical measurement unit 3 obtained when measuring a standard sample of known concentration.
  • absorbance and conductivity it is sufficient to put zero in the pH term in the above equation 1, and when using two explanatory variables, absorbance and pH, the above number In 1, it suffices to put zero in the conductivity term.
  • FIG. 2 shows the effects of machine differences between (a) the case of using the calibration curve of the conventional example and (b) the case of using the calibration curve of the present embodiment.
  • FIG. 2 shows experimental data using a mixed liquid sample containing two components (component A and component B) with known concentrations.
  • each calibration curve of the conventional example was created using only the light absorption spectrum of the absorbance meter, and each calibration curve of the present example is composed of the light absorption spectrum of the absorbance meter, the conductivity of the conductivity meter, and the pH It was created using the pH of the meter. Both "apparatus X" and “apparatus Y” indicate the predicted concentration "ppm" when the same calibration curve is applied.
  • the concentration of the component to be measured is calculated by multivariate analysis using the optical absorption spectrum (spectral spectrum) of the liquid sample and the characteristic values of the liquid sample as explanatory variables.
  • the concentration of the component to be measured can be obtained with high accuracy.
  • characteristic values obtained by electrochemical measurement which is a measurement method with little instrumental difference in principle, are used as explanatory variables for multivariate analysis.
  • concentration of the component to be measured is calculated using only spectroscopy, it is possible to reduce the instrumental difference in the predicted concentration, and it is possible to obtain the concentration of the component to be measured with high accuracy regardless of the device.
  • the values (spectral spectrum and characteristic values) obtained by multiple measurement principles are used as explanatory variables, even if the spectral spectrum of the component to be measured is superimposed on the spectral spectrum of another component, the Concentration can be measured with high accuracy.
  • liquid sample temperature and physical property values of liquid samples measured by measurement principles other than electrochemical measurements can be added. good.
  • either conductivity or pH may be used, and in addition to conductivity or pH, refractive index, viscosity, chromaticity, alkalinity, acidity, ORP, water Hardness, turbidity, density, concentration of ions other than hydrogen ions, etc. may be added.
  • ultrasonic signal intensity, flow rate, pressure, or the like may be added.
  • multivariate analysis is performed using a differential value obtained by differentiating the spectral spectrum as an explanatory variable.
  • the optical measurement unit of the above-described embodiment is of a type in which, for example, the flow cell 21 (sample) is irradiated with white light, and the light transmitted through the flow cell 21 (sample) is spectrally detected.
  • a method may be used in which the light is dispersed before irradiating it onto the flow cell 21 (sample) and the flow cell 21 (sample) is irradiated with the dispersed light, and the wavelength with which the flow cell 21 (sample) is irradiated is changed.
  • the optical measurement unit 2 of the above embodiment is an absorbance meter, it may be of another type for measuring the spectroscopic spectrum of a liquid sample.
  • the optical measurement unit 2 include an ultraviolet/visible spectrophotometer, an infrared spectrophotometer, a Fourier transform infrared spectrophotometer (FTIR), a non-dispersive infrared spectrophotometer (NDIR), and a near-infrared spectrophotometer.
  • FTIR Fourier transform infrared spectrophotometer
  • NDIR non-dispersive infrared spectrophotometer
  • NMR inductively coupled plasma atomic emission spectrometer
  • ICP-AES inductively coupled plasma atomic emission spectrometer
  • XAFS X-ray fluorescence spectrometer
  • NMR nuclear magnetic resonance spectrometer
  • FT-NMR Fourier transform nuclear magnetic resonance spectrometer
  • the concentration of the component to be measured in the liquid sample can be obtained with high accuracy.

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PCT/JP2022/040152 2021-11-22 2022-10-27 成分濃度測定装置、成分濃度測定プログラム、及び、成分濃度測定方法 Ceased WO2023090111A1 (ja)

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CN202280073109.0A CN118215836A (zh) 2021-11-22 2022-10-27 成分浓度测定装置、成分浓度测定程序以及成分浓度测定方法
US18/702,053 US20250044209A1 (en) 2021-11-22 2022-10-27 Component concentration measuring device, component concentration measuring program, and component concentration measuring method
JP2023561498A JPWO2023090111A1 (https=) 2021-11-22 2022-10-27
KR1020247012905A KR20240112258A (ko) 2021-11-22 2022-10-27 성분 농도 측정 장치, 성분 농도 측정 프로그램, 및 성분 농도 측정 방법

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KR102722361B1 (ko) * 2024-06-17 2024-10-25 주식회사 동서라인텍 산 분석이 가능한 ｘｒｆ 분석장치

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JPH1137935A (ja) * 1997-07-18 1999-02-12 Fuji Electric Co Ltd 下水中の複数成分定量方法とその装置
JP2000356635A (ja) * 1999-06-15 2000-12-26 Meidensha Corp クロロフィルａ濃度測定方法及びその装置
JP2002122538A (ja) * 2000-10-17 2002-04-26 National Food Research Institute 近赤外分光法を用いた液状試料の分析法および分析装置
JP2008169094A (ja) * 2007-01-12 2008-07-24 Nara Institute Of Science & Technology カーボンナノチューブ分散液およびその製造方法、並びにその利用
JP2012154698A (ja) * 2011-01-24 2012-08-16 Mitsubishi Heavy Ind Ltd 酸濃度計測装置
JP2020176839A (ja) * 2019-04-15 2020-10-29 株式会社日立製作所 光分析方法および光分析システム

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